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022 _a0021-9584
100 _aHilts, Adrian R.
245 _aImproved Yields of Dichlorobis(triphenylphosphine)nickel(II) and Related Compounds by Employing Triethyl Orthoformate as an In Situ Dehydrating Agent
_b: Rational Improvement of a Classic Undergraduate Inorganic Synthesis (Journal Article)
260 _aWashington DC
_b: American Chemical Society
_c, 2023
300 _a4119–4121p.
440 _aJournal of Chemical Society
_v, Volume 100: Number 10, October 2023
505 _a***______{For Hard Copy, Please visit Library.}________***
520 _aAbstract: The addition of a small excess of triethyl orthoformate to an alcoholic mixture of NiCl2·6H2O and triphenylphosphine (PPh3) results in an increase in the typical isolated yield of [NiCl2(PPh3)2] from below 50% to over 85%. The impact of water when present in the reaction medium in this system is discussed, and results from the application of the same synthetic approach to the syntheses of [NiBr2(PPh3)2], [NiCl2(dppe)], and [NiBr2(dppe)] are presented. A simple synthesis of NiCl2·2H2O by the dehydration of NiCl2·6H2O at 80 °C can be performed as an optional step to decrease the quantity of triethyl orthoformate required for the preparation of [NiCl2(PPh3)2] and/or [NiCl2(dppe)]. The experiments are flexible and accommodate a variety of laboratory schedules and student skill levels. Each synthesis can be readily completed within a 3 h laboratory period.
650 _aInorganic Chemistry| Laboratory Instruction| Hands-On Learning/Manipulatives| Coordination Compounds| Synthesis
700 _aCooke, Jason
856 _uhttps://doi.org/10.1021/acs.jchemed.3c00637
942 _cPER
999 _c45364
_d45363